CN110508231A - The continuous production system of the azo active dyestuff of hypergravity - Google Patents
The continuous production system of the azo active dyestuff of hypergravity Download PDFInfo
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- CN110508231A CN110508231A CN201910711393.XA CN201910711393A CN110508231A CN 110508231 A CN110508231 A CN 110508231A CN 201910711393 A CN201910711393 A CN 201910711393A CN 110508231 A CN110508231 A CN 110508231A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/82—Combinations of dissimilar mixers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
- B01J19/243—Tubular reactors spirally, concentrically or zigzag wound
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B62/00—Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves
- C09B62/44—Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves with the reactive group not directly attached to a heterocyclic ring
- C09B62/503—Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves with the reactive group not directly attached to a heterocyclic ring the reactive group being an esterified or non-esterified hydroxyalkyl sulfonyl or mercaptoalkyl sulfonyl group, a quaternised or non-quaternised aminoalkyl sulfonyl group, a heterylmercapto alkyl sulfonyl group, a vinyl sulfonyl or a substituted vinyl sulfonyl group, or a thiophene-dioxide group
- C09B62/507—Azo dyes
- C09B62/51—Monoazo dyes
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Abstract
The present invention provides the continuous production system of the azo active dyestuff of hypergravity, by spiral coil reactor in conjunction with high-gravity technology, diazo-reaction and coupling reaction differentiation are treated, diazo-reaction carries out in spiral coil reactor, and supergravity reactor can largely improve the quality of conversion ratio and product for coupling reaction.And spiral coil reactor being capable of accurate temperature controlling, avoid the decomposition of diazonium salt, under cooperating in this way, since temperature control is accurate, diazonium salt decomposes seldom, will not influence the progress of subsequent coupling reaction, therefore can guarantee that the concentration of diazonium salt when continuous production maintains higher range, it is close or identical with a batch of azo active dyestuff performance so as to guarantee, adapt to the actual demand of industry.Further, the setting disturbance part in spiral coil, can disturb the reaction solution in the spiral coil reactor, accelerate the flowing and mixing of reaction solution, be conducive to homogenization reaction.
Description
Technical field
The present invention relates to azo active dyestuff preparation technical fields.More particularly, to a kind of azo of hypergravity
The continuous production system of reactive dye.
Background technique
Industrially, the production of reactive azo dyes is to be carried out in stirred tank reactor with andnon-continuous operation manner.By
Too big in the complexity and stirred tank reactor volume of organic reaction, the temperature and mixed effect for leading to material are in partial zones
Domain is difficult to reach uniformly, and the production efficiency of dyestuff is low, and difference is larger between the dyestuff each batch of batch agitator kettle production, right
The post-processing of dyestuff and the application of dyestuff all bring inconvenience.
Therefore, it is urgent to provide a kind of continuous production systems of the azo active dyestuff of hypergravity.
Summary of the invention
In view of this, in order to solve the continuous production system for lacking effective azo active dyestuff at present, the present invention is mentioned
For a kind of continuous production system of the azo active dyestuff of hypergravity.
In certain embodiments, a kind of continuous production system of the azo active dyestuff of hypergravity, the system
Include:
Condensation reaction unit, the condensation reaction unit includes condensation reaction tank, for generating coupling component；
Diazo-reaction unit, the diazo-reaction unit include:
Component is premixed, diazo component and diazo reagent are premixed, and
Spiral coil reactor is connected to the premix component, so that the reaction solution after premix is in the spiral coil
Diazo-reaction is carried out in reactor generates diazonium salt；
The system further comprises:
The hypergravity coupling reaction unit being connected with the diazo-reaction unit and the condensation reaction unit, it is described
Hypergravity coupling reaction unit generates the idol for making diazonium salt and coupling component carry out coupling reaction under Elevated Gravity
Nitrogen reactive dye；
Wherein, the disturbance part of fixed structure is provided in the inner cavity of the spiral coil reactor generation diazo-reaction,
The disturbance part is used to disturb the reaction solution in the spiral coil reactor.
In certain embodiments, the disturbance part includes the fixation being fixed on the spiral coil reactor surface of internal cavity
Portion, and fixed freedom portion in conjunction with the one end of the fixed part far from the spiral coil reactor surface of internal cavity, it is described
Freedom portion includes two, and two freedom portion and the fixed part constitute Y-shaped structure or T-shape structure.
In certain embodiments, the disturbance part is vertically arranged with the spiral coil reactor surface of internal cavity, Huo Zheqing
Tiltedly setting.
In certain embodiments, the disturbance part includes first part along feed liquor direction undergauge, and with described first
The second part of the lesser one end connection of partial internal diameter, the second part is in expanding structure along feed liquor direction, and described
First part and the second part are symmetrical arranged by symmetrical plane of its joint face.
In certain embodiments, the system further comprises:
Ultrasonic feed-in device, for respectively to the spiral coil reactor and the hypergravity coupling reaction unit feed-in
Ultrasound, wherein identical with the ultrasound intensity of the hypergravity coupling reaction unit feed-in or not to the spiral coil reactor
Together.
In certain embodiments, the premix component includes the first perfusion tube and the second perfusion tube；
First perfusion tube is sheathed on the outside of second perfusion tube, and first perfusion tube and described second
Cavity with gap for one of circulation of diazo component and diazo reagent between perfusion tube, in second perfusion tube
It circulates for the another one of diazo component and diazo reagent；
First perfusion tube forms mixed for diazo component and diazo reagent close to one end of the spiral coil reactor
The pre-mix zone of conjunction, second perfusion tube extends to the inlet of the pre-mix zone, and sprays the diazonium to the pre-mix zone
The another one of component and diazo reagent.
In certain embodiments, the pre-mix zone includes closing on the reducing diameter part of its inlet and integrally connecting with the reducing diameter part
Logical flat part.
In certain embodiments, the hypergravity coupling reaction unit includes:
Supergravity reactor is connected to the spiral coil reactor；
Stirred tank reactor is connected with the supergravity reactor, and
Pump and stirred tank for the diazonium salt after diazo reaction to be pumped into the high gravity rotating packed bed reactor is anti-
Device discharge port circulation is answered to return the pump of supergravity reactor.
In certain embodiments, the system further comprises heat exchange unit, and the heat exchange unit is for controlling the spiral shell
The intracorporal temperature of capstan pipe reactor reaction chamber and the intracorporal temperature of the hypergravity coupling reaction unit process chamber.
In certain embodiments, the heat exchange unit includes:
It is set in the pipeline collet of the pipeline external of the spiral coil reactor, the pipeline collet has and can be passed through liquid
The cavity of body；
It is set in the shell collet that the supergravity reactor forms the outer side of shell of reaction cavity, the shell collet tool
There is the cavity that can be passed through liquid；And
For the heat-exchanger rig for being passed through liquid in the pipeline collet and the shell collet to be heated or cooled.
Beneficial effects of the present invention are as follows:
The present invention provide hypergravity azo active dyestuff continuous production system, by spiral coil reactor with
High-gravity technology combines, and diazo-reaction and coupling reaction differentiation is treated, diazo-reaction is in spiral coil reactor
It carries out, supergravity reactor can largely improve the quality of conversion ratio and product for coupling reaction.And helical disk
Pipe reactor can accurate temperature controlling, avoid the decomposition of diazonium salt, under cooperating in this way, since temperature control is accurate, diazonium salt is decomposed
Seldom, will not influence the progress of subsequent coupling reaction, thus can guarantee the concentration of diazonium salt when continuous production maintain compared with
High range, it is close or identical with a batch of azo active dyestuff performance so as to guarantee, adapt to the actual demand of industry.
Further, the setting disturbance part in spiral coil, can disturb the reaction solution in the spiral coil reactor, accelerate anti-
The flowing and mixing for answering solution are conducive to homogenization reaction.
Detailed description of the invention
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing.
The continuous production system structure that Fig. 1 shows the azo active dyestuff of the hypergravity in the embodiment of the present invention is shown
It is intended to.
Fig. 2 shows the structural schematic diagrams of the premix component in the embodiment of the present invention.
Fig. 3 a shows one of the structural schematic diagram of the disturbance part in the embodiment of the present invention in spiral coil inner cavity.
Fig. 3 b shows the second structural representation of the disturbance part in the embodiment of the present invention in spiral coil inner cavity.
Fig. 3 c shows the third structural representation of the disturbance part in the embodiment of the present invention in spiral coil inner cavity.
Fig. 3 d shows the four of the structural schematic diagram of the disturbance part in the embodiment of the present invention in spiral coil inner cavity.
Specific embodiment
In order to illustrate more clearly of the present invention, the present invention is done further below with reference to preferred embodiments and drawings
It is bright.Similar component is indicated in attached drawing with identical appended drawing reference.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
In view of this, present invention firstly provides a kind of continuous production system of the azo active dyestuff of hypergravity,
The system comprises: condensation reaction unit, the condensation reaction unit includes condensation reaction tank, for generating coupling component；Weight
Nitridation reaction unit, the diazo-reaction unit includes: premix component, is premixed to diazo component and diazo reagent, and
Spiral coil reactor is connected to the premix component, make premix after reaction solution in the spiral coil reactor into
Row diazo-reaction generates diazonium salt；The system further comprises: with the diazo-reaction unit and the condensation reaction
The hypergravity coupling reaction unit that unit is connected, the hypergravity coupling reaction unit is for making diazonium under Elevated Gravity
Salt and coupling component carry out coupling reaction and generate the azo active dyestuff；Wherein, diazonium occurs for the spiral coil reactor
Change the disturbance part that fixed structure is provided in the inner cavity of reaction, the disturbance part is for disturbing in the spiral coil reactor
Reaction solution.
The continuous production system of above-mentioned azo active dyestuff provided by the invention is answered using spiral coil reactor first
It,, can be with when needing temperature to control since the reaction chamber of coil reactor is helical disk tubulose for diazo-reaction
Heat medium or cooling medium are passed through in the collet for being set in coil pipe outer wall, the pipe diameter of spiral coil is small, tube wall
It is relatively thin, therefore heat directly can be conducted or be removed by metal pipe-wall in a very short period of time by the collet being arranged on outer side wall
Reaction system, and caliber is small, and it is uniform to manage intracorporal reaction solution heat transfer, thus achieve the purpose that accurate temperature controlling, Neng Gouzhun
The lifting of true control system temperature, largely reduces the decomposition of diazonium salt.
In addition, the present invention is further by spiral coil reactor in conjunction with high-gravity technology, for diazo-reaction and idol
It closes reaction differentiation to treat, diazo-reaction carries out in spiral coil reactor, and supergravity reactor can for coupling reaction
Largely improve the quality of conversion ratio and product.And spiral coil reactor can accurate temperature controlling, avoid diazonium salt
It decomposes, the two combines, and since temperature control is accurate, diazonium salt is decomposed seldom, it will not influence the progress of subsequent coupling reaction,
Therefore it can guarantee that the concentration of diazonium salt when continuous production maintains higher range, so as to guarantee with a batch of azo
Reactive dye performance is close or identical, adapts to the actual demand of industry.
Again, part is disturbed by setting, improves the mixing of reaction solution in coil pipe, while accelerating reaction speed, favorably
It is reacted in homogenization.
In some embodiments, supergravity reactor can select such as rotary packed bed, rotor, deflector type, spiral
The hypergravities rotating devices such as channel, rotating compact disc formula, wherein rotary packed bed includes shell, rotation chamber, and rotation chamber passes through
Motor drives rotation, is provided with filler in rotating drum room, and filler is used to for liquid being cut into the infinitesimal (drop or) of micro/nano-scale
Such as wire packing etc., the invention is not limited in this regard.Rotor is with rotary packed bed the difference is that being determined by fixed
Cutting between sub- column and the rotor of rotation, and then liquid is cut into the infinitesimal (drop or liquid film) of micro/nano-scale.
Further, in a preferred embodiment, the system further comprises: ultrasonic feed-in device, for respectively to institute
State spiral coil reactor and hypergravity coupling reaction unit feed-in ultrasound, wherein to the spiral coil reactor and
The ultrasound intensity of the hypergravity coupling reaction unit feed-in is identical or different.
It, can be with flow-disturbing ring in combination with ultrasound since disturbance part makes reaction liquid form flow-disturbing environment in coil pipe
The micromixing in border cooperates, and further realizes microcosmic mixing by molecular vibration, so the mixing of both macro and micro simultaneously into
Row further achievees the effect that mass transfer mixes, at the same time, since coil pipe caliber is smaller, reaction solution higher for viscosity
Or slurries, the phenomenon that setting of part is easy to cause Partial Blocking is disturbed, cooperation ultrasound can be by molecular vibration, so that molecule
It will not be stopped in fixed position, significantly reduce clogging, accelerate the flowing of reaction solution or slurries.
In a specific embodiment, as shown in Figure 1, Fig. 1 shows a kind of continuous process system, the continuous process system
It include: diazo component blending tank 1, diazo reagent head tank 2, pump 3, pump 4, premix component 5, spiral coil reactor 7, coupling group
Divide head tank 9, supergravity reactor 11, collection container 14.Wherein, diazo component blending tank 1 is connected by pump 3 and premix component 5
It is logical, so that diazo component is passed through premix component 5.Diazo reagent head tank 2 is connected to by pump 4 with premix component 5, to will weigh
Nitrogen reagent is passed through premix component 5, and then in premix component 5, diazo component and diazo reagent mixing.Premix component 5 and spiral
Coil reactor 7 is connected to, and the diazo component mixed and diazo reagent are passed through in spiral coil reactor 7 and carried out instead
It answers, supergravity reactor 11 is entered after diazo reaction and carries out coupling reaction, the product after coupling reaction enters collection container
In 14.
Include supergravity reactor 11 in the embodiment, can be used for diazo-reaction-coupling reaction continuous production.Example
Such as red reactive azo dyes active red M-3BE.
In some embodiments, as shown in Fig. 3 a to Fig. 3 d, the disturbance part includes being fixed on the spiral coil reaction
Fixed part on device surface of internal cavity, and in conjunction with the one end of the fixed part far from the spiral coil reactor surface of internal cavity
Fixed freedom portion, the freedom portion include two, two freedom portion and the fixed part constitute Y-shaped structure or
T-shape structure.
Further, as can be seen that the disturbance part and spiral coil reactor inner cavity table from Fig. 3 a to Fig. 3 d
Face is vertically arranged, or is obliquely installed.
Specifically, in conjunction with above-mentioned diagram, the disturbance part includes the first part along feed liquor direction undergauge, and with it is described
The second part of the lesser one end connection of the internal diameter of first part, the second part is in expanding structure along feed liquor direction, and
The first part and the second part are symmetrical arranged by symmetrical plane of its joint face.
In some embodiments, above system further comprises heat exchange unit, and spiral can be heated or cooled in heat exchange unit
The tube body of coil reactor, such as the tube wall of spiral coil reactor are arranged with heat exchange jacket (not shown).Due to
Pipe diameter is small, therefore thermal energy or cold energy rapidly can be diffused to equably and entirely be managed in intracorporal cavity by heat exchange jacket.
In some embodiments, the spiral coil in the spiral coil reactor is made of polyurethane.It in this way can be with
It prevents from corroding, while heat transfer is influenced smaller.
Certainly, as embodiment unlike this embodiment, spiral coil in the spiral coil reactor it is interior
Surface is lined with urethane material.
Equally, in order to avoid the influence of corrosion, above-mentioned pump is polytetrafluoro constant-flux pump.
In some preferred embodiments, the heat exchange unit includes being set in outside the pipeline of the spiral coil reactor
The pipeline collet in portion, the pipeline collet have the cavity that can be passed through liquid；The pipe is passed through with for heating or cooling medium
The heat-exchanger rig of liquid in road collet,.Spiral coil reactor tube body is heated or cooled by liquid to realize temperature
It is precisely controlled.
In addition, the heating or cooling medium in pipeline collet can be water, alcohol, salting liquid, or oil, the present invention
It is without limitation.
In the above-described embodiments, the specific structure of component is premixed as shown in Fig. 2, the premix component includes the first perfusion tube
51 (outer layer perfusion tubes) and the second perfusion tube 52 (internal layer perfusion tube)；First perfusion tube 51 is sheathed on second perfusion tube
52 outside, and have gap for diazo component and diazonium between first perfusion tube 51 and second perfusion tube 52
One of circulation of reagent, the another one stream of cavity in second perfusion tube 52 for diazo component and diazo reagent
It is logical；First perfusion tube 51 is mixed close to the formation of one end of the spiral coil reactor for diazo component and diazo reagent
Pre-mix zone 53, second perfusion tube 52 extend to the inlet of the pre-mix zone 53, and spray to the pre-mix zone 53 described
The another one of diazo component and diazo reagent.When it is implemented, the sky between the first perfusion tube 51 and the second perfusion tube 52
Clearance flow leads to diazo component, and circulate diazo reagent in the second perfusion tube 52, and certainly, in other embodiments, vice versa, the present invention
It is without limitation.
It should be noted that the charging of the first perfusion tube 51 is feeding vertical, feed inlet is formed in tube wall, and then keep away
Exempt from the first perfusion tube 51 and the second perfusion tube 52 and leads to not asking for charging from same position (left position in diagram) charging
Topic.
Further, in order to make by premix component outflow solution have faster speed, the pre-mix zone
Including the flat part for closing on the reducing diameter part of its inlet and being integrally connected to the reducing diameter part.In this way discharging when liquid outlet
Bore becomes smaller, and can accelerate the speed for flowing out solution.
It is very close to each other between heat exchange jacket and the tube wall of spiral coil reactor in some preferred embodiments,
This avoid the air of low heat transfer rate to have an impact to heat transfer.
Diazo-reaction occurs in spiral coil reactor, diazonium salt is generated, since spiral coil reactor can be accurate
Control temperature, therefore can be avoided the decomposition of diazonium salt so that in a batch of continuous production diazonium salt it is subsequent into
Material concentration holding is stablized constant, so that stable product quality, differs smaller with a batch of properties of product.
In some embodiments, supergravity reactor can be rotating packed bed reactor or rotor reactor,
Those skilled in the art are illustrated, and the present invention with no restrictions, as needed, can arbitrarily set the concrete type of supergravity reactor
Set the one of which of all supergravity reactors in the prior art.
It should be noted that the liquid distribution trough of supergravity reactor is two bursts of chargings in diagram in the present embodiment, point
It does not spray, but in other embodiments, pre-mix zone can also be set at liquid distribution trough jet port, and then before ejecting,
Diazonium salt solution and coupling component enter supergravity reactor first in liquid each by the first liquid-inlet and second liquid import
The pre-mix zone of body distributor is premixed, and then into reaction inner cavity, the present invention does not do further limitation to this for injection.
It should be noted that coupling reaction also needs to guarantee certain temperature, but compared to diazo-reaction for, it is even
It is not high to the demand for control of temperature to close reaction, is experimentally confirmed, for coupling reaction using supergravity reactor compared to spiral shell
Capstan pipe reactor has more advantage.
In addition, since coupling reaction needs to guarantee certain temperature, it can be anti-to hypergravity by above-mentioned heat exchange unit
The shell of device is answered to be heated or cooled, to realize the control to temperature.
In certain embodiments, heat exchange unit further comprises being set in the supergravity reactor to form reaction chamber
The shell collet of body, shell collet have the cavity that can be passed through liquid.Further, heat-exchanger rig can be heated or cooled simultaneously
Liquid in pipeline collet and shell collet.Further, pipeline collet is connected to shell collet, and heat transferring medium can be from pipe
Road collet flows into shell collet, without limitation.
In certain embodiments, the diazo component includes 2- naphthylamines -1,5 disulfonic acid, the diazo reagent packet
Nitrite and hydrochloric acid are included, the coupling component includes that H acid, para-ester and Cyanuric Chloride are condensed resulting condensation liquid twice, this
Sample is red reactive azo dyes active red M-3BE by the azo active dyestuff that above system of the invention generates.
Certainly, continuous process system of the invention is not limited to above two specific embodiment, it is to be understood that this system
It can be suitable for any azo active dyestuff for carrying out diazo-reaction and coupling reaction, the present invention does not do exhaustion herein.
System is generated to serialization provided by the invention below with reference to two specific examples to be described in detail.
Red reactive azo dyes active red M-3BE serialization generates
In the embodiment, the diazo component includes 2- naphthylamines -1,5 disulfonic acid, the diazo reagent include hydrochloric acid and
Sodium nitrite, the coupling component include that H acid, para-ester and Cyanuric Chloride are condensed resulting condensation liquid twice.
Diazo-reaction process are as follows: 2- naphthylamines -1,5 disulfonic acid and nitrite mixed liquor and hydrochloric acid solution are passed through into premix
Component is premixed, as shown in Fig. 2, being then continuously input into spiral coil reactor respectively by pipeline, is followed again in exit
Ring returns helix tube entrance, obtains diazonium salt suspension, and diazo-reaction is at -10 DEG C to+40 DEG C, at preferably 0 DEG C to 12 DEG C
It carrying out, the molar ratio of the hydrogen ion of diazo-reaction hydrochloric acid and 2- naphthylamines -1,5 disulfonic acid is 2.5~4:1 when charging, preferably 3:
1, the molar ratio of sodium nitrite and para-ester is 1~2:1, preferably 1.01~1.1:1, and feed flow rate is excellent in 0.08~0.8m/s
Select 0.25~0.7m/s.
Condensation reaction are as follows: Cyanuric Chloride and H acid are passed through in stirred tank at 0-5 DEG C of temperature by constant flow pump, pH is
2.5~3.5 it is lower carry out primary condensation reactions, be passed through para-ester and primary condensation liquid again after reaction at 30-35 DEG C of temperature, pH
Progress secondary condensation obtains secondary condensation liquid and is coupled material liquid under the conditions of being 3~4.
Coupling reaction process are as follows: diazonium salt and coupling component are continuously input into rotating packed bed reactor respectively, passed through
Hybrid reaction generates azo-compound, and reaction temperature is 0 DEG C to 45 DEG C, preferably 8 DEG C~15 DEG C；, preferred pH=6~8.5；It is overweight
Power reactor revolving speed is 1200~3200rpm, preferably 1600~1900rpm.
Below using certain specific experiment parameters as example, to the red of continuous production method production through the invention
The performance of reactive azo dyes active red M-3BE is illustrated.
(a) preparation (spiral coil reactor) of 2- naphthylamines -1,5 disulfonic acid diazonium salt
It weighs 6.40g2- naphthylamines -1,5 disulfonic acid and adds water 90ml, then plus 10%Na2CO3Solution stirring, room-temperature dissolution to pH
=6~6.5, add 1.1178gNaNO2 stirring and dissolving, referred to as 2- naphthylamines -1,5 disulfonic acid and sodium nitrite mixed liquor liquid measure
About 105ml.
The hydrochloric acid that 2- naphthylamines -1,5 disulfonic acid and sodium nitrite mixed liquor and 45ml concentration are 1mol/L is passed through into peristaltic pump
Squeeze into the premix component of spiral coil reactor.Temperature is controlled by thermostat collet at 8 DEG C.Obtain faint yellow 2- naphthylamines -1,5 two
Sulfonic acid diazonium salt suspension.
(b) preparation (stirred tank reactor) of coupling component
The para-ester powder for weighing 4.45g, adds water 30ml, adds 10%Na2CO3Solution stirring, room-temperature dissolution to pH=
6~6.5, then filtered to obtain para-ester sodium salt solution；5.63g H acid powder is weighed, adds water 30ml, adds 10%
Na2CO3Solution stirring, room-temperature dissolution to pH=6~6.5 obtain H acid double sodium salt solution；Cyanuric Chloride powder 2.83g is weighed, directly
It connects and pours into stirred tank reactor, add ice water mixed solution 72ml, Cyanuric Chloride is beaten at 0~5 DEG C, then pass through constant current
H acid is passed through in stirred tank by pump carries out primary condensation reaction, to after reaction, be passed through again by constant flow pump by ester solution is aligned
In stirred tank, secondary condensation is carried out at 30~35 DEG C, is obtained secondary condensation liquid and is coupled material liquid.
(c) coupling reaction (supergravity reactor)
It obtains secondary condensation liquid by above-mentioned and is connect with one of entrance of coupling reaction revolving bed, spiral coil is reacted
Device outlet is connect with another high-gravity rotating bed entrance, is divided to two stock materials to enter high-gravity rotating bed middle reaction, is entered back into
Circulation returns supergravity reactor after stirred tank reactor, and temperature is controlled by thermostat collet at 10 DEG C or so, revolving bed revolving speed
For 1700rpm, red coupling product is obtained.
Feed liquid is saltoutd, is dried, purification, then after drying, active red M-3BE dyestuff is obtained, yield is up to 96%, sample
Product purity is up to 92%.
Obviously, the product in this experiment scene can reach the sample with high-purity in high yield, and with a batch of production
Moral character can be almost the same, certainly, although the present invention is using red reactive azo dyes active red M-3BE showing as continuous production
Example, but not indicate that the present invention can be only used to above-mentioned example, from the point of view of inventive concept of the invention, azo active dyestuff
Type and main body of the invention design have no direct correlation.It is to be understood that those of ordinary skill in the art combine this hair
The inventive concept of bright proposition can be applied in any azo active dyestuff, and the present invention does not do exhaustion herein.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention may be used also on the basis of the above description for those of ordinary skill in the art
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is all to belong to this hair
The obvious changes or variations that bright technical solution is extended out are still in the scope of protection of the present invention.
Claims (10)
1. a kind of continuous production system of the azo active dyestuff of hypergravity, which is characterized in that the system comprises:
Condensation reaction unit, the condensation reaction unit includes condensation reaction tank, for generating coupling component；
Diazo-reaction unit, the diazo-reaction unit include:
Component is premixed, diazo component and diazo reagent are premixed, and
Spiral coil reactor is connected to the premix component, so that the reaction solution after premix is reacted in the spiral coil
Diazo-reaction is carried out in device generates diazonium salt；
The system further comprises:
The hypergravity coupling reaction unit being connected with the diazo-reaction unit and the condensation reaction unit is described overweight
It is living for making diazonium salt and coupling component carry out the coupling reaction generation azo under Elevated Gravity that couple closes reaction member
Property dyestuff；
Wherein, the disturbance part of fixed structure is provided in the inner cavity of the spiral coil reactor generation diazo-reaction, it is described
Disturbance part is used to disturb the reaction solution in the spiral coil reactor.
2. system according to claim 1, which is characterized in that the disturbance part includes being fixed on the spiral coil reaction
Fixed part on device surface of internal cavity, and in conjunction with the one end of the fixed part far from the spiral coil reactor surface of internal cavity
Fixed freedom portion, the freedom portion include two, two freedom portion and the fixed part constitute Y-shaped structure or
T-shape structure.
3. system according to claim 2, which is characterized in that the disturbance part and spiral coil reactor inner cavity table
Face is vertically arranged, or is obliquely installed.
4. system according to claim 1, which is characterized in that the disturbance part includes along first of feed liquor direction undergauge
Divide, and the second part being connected to the lesser one end of the internal diameter of the first part, the second part are in along feed liquor direction
Expanding structure, and the first part and the second part are symmetrical arranged by symmetrical plane of its joint face.
5. system according to claim 1, which is characterized in that the system further comprises:
Ultrasonic feed-in device, for super to the spiral coil reactor and the hypergravity coupling reaction unit feed-in respectively
Sound, wherein the ultrasound intensity to the spiral coil reactor and the hypergravity coupling reaction unit feed-in is identical or different.
6. system according to claim 1, which is characterized in that the premix component includes the first perfusion tube and the second infusion
Pipe；
First perfusion tube is sheathed on the outside of second perfusion tube, and first perfusion tube and second infusion
With gap for one of circulation of diazo component and diazo reagent between pipe, the cavity in second perfusion tube is for weight
Nitrogen component and the circulation of the another one of diazo reagent；
First perfusion tube is mixed close to the formation of one end of the spiral coil reactor for diazo component and diazo reagent
Pre-mix zone, second perfusion tube extends to the inlet of the pre-mix zone, and sprays the diazo component to the pre-mix zone
With the another one of diazo reagent.
7. system according to claim 6, which is characterized in that the pre-mix zone include close on its inlet reducing diameter part and
The flat part being integrally connected to the reducing diameter part.
8. system according to claim 1, which is characterized in that the hypergravity coupling reaction unit includes:
Supergravity reactor is connected to the spiral coil reactor；
Stirred tank reactor is connected with the supergravity reactor, and
For the diazonium salt after diazo reaction to be pumped into the pump and stirred tank reactor of the high gravity rotating packed bed reactor
Discharge port recycles the pump for returning supergravity reactor.
9. system according to claim 1, which is characterized in that the system further comprises heat exchange unit, the heat exchange
Unit is for controlling the intracorporal temperature of the spiral coil reactor reaction chamber and the hypergravity coupling reaction unit process chamber
Intracorporal temperature.
10. system according to claim 9, which is characterized in that the heat exchange unit includes:
It is set in the pipeline collet of the pipeline external of the spiral coil reactor, the pipeline collet has and can be passed through liquid
Cavity；
It is set in the shell collet that the supergravity reactor forms the outer side of shell of reaction cavity, the shell collet has can
It is passed through the cavity of liquid；And
For the heat-exchanger rig for being passed through liquid in the pipeline collet and the shell collet to be heated or cooled.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111589394A (en) * | 2020-06-30 | 2020-08-28 | 江苏京控装备有限公司 | Ultrasonic homogeneous single-tube reactor |
| CN112457683A (en) * | 2020-11-26 | 2021-03-09 | 北京化工大学 | Continuous production system of nanometer azo-dye |
| CN112592602A (en) * | 2020-11-04 | 2021-04-02 | 北京化工大学 | Continuous production system of nano disperse dye |
| CN113181814A (en) * | 2021-03-12 | 2021-07-30 | 北京化工大学 | A hypergravity reaction system for oil-solid separation |
| WO2021191497A1 (en) * | 2020-03-24 | 2021-09-30 | Lappeenrannan-Lahden Teknillinen Yliopisto Lut | An ultrasound processing device |
| CN114410122A (en) * | 2021-12-23 | 2022-04-29 | 上海染料研究所有限公司 | Method for synthesizing tartrazine by micro-channel continuous flow and product thereof |
| CN114425260A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | Liquid-liquid mixing device and mixing method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101870824A (en) * | 2010-06-08 | 2010-10-27 | 北京化工大学 | Method for preparing azo colouring agent by utilizing supergravity reactor |
-
2019
- 2019-08-02 CN CN201910711393.XA patent/CN110508231B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101870824A (en) * | 2010-06-08 | 2010-10-27 | 北京化工大学 | Method for preparing azo colouring agent by utilizing supergravity reactor |
Non-Patent Citations (2)
| Title |
|---|
| 苏为科，余志群: "连续流反应技术开发及其在制药危险工艺中的应用", 《中国医药工业杂志》 * |
| 赵东波: "流动化学在药物合成中的最新进展", 《有机化学》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021191497A1 (en) * | 2020-03-24 | 2021-09-30 | Lappeenrannan-Lahden Teknillinen Yliopisto Lut | An ultrasound processing device |
| CN111589394A (en) * | 2020-06-30 | 2020-08-28 | 江苏京控装备有限公司 | Ultrasonic homogeneous single-tube reactor |
| CN114425260A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | Liquid-liquid mixing device and mixing method |
| CN112592602A (en) * | 2020-11-04 | 2021-04-02 | 北京化工大学 | Continuous production system of nano disperse dye |
| CN112592602B (en) * | 2020-11-04 | 2022-06-28 | 北京化工大学 | Continuous production system of nano disperse dye |
| CN112457683A (en) * | 2020-11-26 | 2021-03-09 | 北京化工大学 | Continuous production system of nanometer azo-dye |
| CN113181814A (en) * | 2021-03-12 | 2021-07-30 | 北京化工大学 | A hypergravity reaction system for oil-solid separation |
| CN114410122A (en) * | 2021-12-23 | 2022-04-29 | 上海染料研究所有限公司 | Method for synthesizing tartrazine by micro-channel continuous flow and product thereof |
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